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    • 102. 发明申请
    • Acid-labile isotope-coded extractant (ALICE) and its use in quantitative mass spectrometric analysis of protein mixtures
    • 酸不稳定同位素编码提取物(ALICE)及其在蛋白质混合物的定量质谱分析中的应用
    • US20050014278A1
    • 2005-01-20
    • US10919365
    • 2004-08-17
    • Yongchang QiuJack WangRodney Hewick
    • Yongchang QiuJack WangRodney Hewick
    • G01N27/62C07D405/12G01N1/28G01N30/46G01N30/72G01N30/88G01N33/532G01N33/58G01N33/68G01N33/00
    • G01N33/6848C07D405/12G01N30/461G01N30/463G01N30/468G01N30/7233G01N33/532G01N33/58G01N33/6803Y10T436/10Y10T436/105831Y10T436/13Y10T436/24Y10T436/25125B01D15/362B01D15/325
    • The method of the invention provides novel compounds, termed acid-labile isotope-coded extractants (ALICE), for quantitative mass spectrometric analysis of protein mixtures. The compounds contain a thiol-reactive group that is used to capture cysteine-containing peptides from all peptide mixtures, an acid-labile linker, and a non-biological polymer. One of the two acid-labile linkers is isotopically labeled and therefore enables the direct quantitation of peptides/proteins through mass spectrometric analysis. Because no functional proteins are required to capture peptides, a higher percentage of organic solvent can be used to solubilize the peptides, particularly hydrophobic peptides, through the binding, washing and eluting steps, thus permitting much better recover of peptides. Moreover, since the peptides are covalently linked to the non-biological polymer (ALICE), more stringent washing is allowed in order to completely remove non-specifically bound species. Finally, peptides captured by ALICE are readily eluted from the polymer support under mild acidic condition with high yield and permit the direct down stream mass spectrometric analysis without any further sample manipulation. In combination with our novel dual column two dimensional liquid chromatography- mass spectrometry (2D-LC-MS/MS) design, the ALICE procedure proves to a general approach for quantitative mass spectrometric analysis of protein mixtures with better dynamic range and sensitivity.
    • 本发明的方法提供了新的化合物,称为酸不稳定同位素编码的提取物(ALICE),用于蛋白质混合物的定量质谱分析。 该化合物含有硫醇反应性基团,其用于从所有肽混合物,酸不稳定接头和非生物聚合物捕获含半胱氨酸的肽。 两个酸不稳定接头之一是同位素标记的,因此能够通过质谱分析直接定量肽/蛋白质。 由于不需要功能蛋白来捕获肽,所以可以使用较高百分比的有机溶剂来通过结合,洗涤和洗脱步骤来增溶肽,特别是疏水性肽,因此可以更好地恢复肽。 此外,由于肽与非生物聚合物(ALICE)共价连接,所以允许更严格的洗涤以完全除去非特异性结合的物质。 最后,ALICE捕获的肽在温和的酸性条件下以高产率容易地从聚合物载体上洗脱,并允许直接的下游质谱分析,无需进一步的样品操作。 结合我们的双柱二维液相色谱 - 质谱(2D-LC-MS / MS)设计,ALICE方法证明了具有更好的动态范围和灵敏度的蛋白质混合物的定量质谱分析的一般方法。
    • 103. 发明授权
    • Protection of the chromatographic bed in dynamic axial compression chromatography devices
    • 动态轴向压缩色谱装置中色谱床的保护
    • US06843918B2
    • 2005-01-18
    • US10366689
    • 2003-02-14
    • Wilhelm HauckHarlene MarksJean BlehautRoger Marc Nicoud
    • Wilhelm HauckHarlene MarksJean BlehautRoger Marc Nicoud
    • G01N27/22B01D15/08B01J20/291G01N30/46G01N30/52G01N30/60G01N30/80G01N30/88
    • B01D15/08G01N30/52G01N30/6004G01N30/6021G01N2030/522G01N30/62
    • The invention relates to a chromatography device comprising: a column (12) intended to house, between its two ends (16a, 16b) a chromatographic bed (14) and a fluid to be chromatographed, a fluid layer (48) being defined between a surface of the bed (14) and one (16a) of the ends of the column (12); a piston (36) sliding in the column (12), the piston (36) being one of the ends (16a, 16b) of the column (12); at least a first probe (45, 46) for detecting the surface of the bed (14), the probe (45, 46) being mounted on the end (16a) of the column (12) defining the layer (48); and means (52) for adjusting the position of the piston (36) according to the detection of the surface of the bed (14) by the probe (45, 46). The invention also relates to processes for separating at least two compounds of a fluid to be chromatographed and to methods of adjusting the position of the piston with respect to the surface of the chromatographic bed using the chromatography device.The invention has the advantage of allowing effective separation of the compounds of the fluid to be chromatographed while ensuring that the bed is protected.
    • 本发明涉及一种色谱装置,其包括:用于在其两端(16a,16b)之间容纳色谱床(14)和要进行色谱分离的流体的柱(12),流体层(48)定义在 床(14)的表面和柱(12)的端部的一个(16a);活塞(36),其在柱(12)中滑动,活塞(36)是其中一个端部(16a,16b) 至少一个用于检测床(14)的表面的第一探针(45,46),探针(45,46)安装在柱(12)的端部(16a)上,所述探针(45,46)限定 层(48); 和用于通过探针(45,46)检测床(14)表面的活塞(36)的位置的装置(52)。本发明还涉及用于分离至少两种化合物 待层析的流体和使用色谱装置调节活塞相对于色谱床表面的位置的方法。本发明的优点在于允许有效分离要进行色谱分离的流体的化合物,同时确保 床被保护。
    • 105. 发明授权
    • Process for recovering betaine
    • 回收甜菜碱的方法
    • US6099654A
    • 2000-08-08
    • US367690
    • 1999-08-19
    • Kikuzo KanekoTakayuki MasudaFumihiko MatsudaKohei SatoKouji Tanikawa
    • Kikuzo KanekoTakayuki MasudaFumihiko MatsudaKohei SatoKouji Tanikawa
    • B01D15/08C07C227/28C07C227/40C07C227/42C07C229/02C07C229/12G01N30/46G01N30/88C07B63/00
    • C07C227/42C07C227/28
    • A starting solution material in the form of waste produced in the course of separation and recovery of sucrose from sugar beet extract or sugar beet molasses with a 2-component separation simulated moving bed chromatographic separator (using a strongly acidic cation exchange resin in a salt form as chromatographic packing) or its concentrate is used to separate therefrom a crude betaine fraction with a 2-component separation simulated moving bed chromatographic separator using as chromatographic packing a strongly acidic cation exchange resin in an ionic form equilibrated with that of the starting solution material. The crude betaine fraction or its concentrate is used to separate therefrom a betaine fraction with a 2-component separation simulated moving bed chromatographic separator using as chromatographic packing a strongly acidic cation exchange resin having at least 10% (based on the ion exchange capacity) of the ionic form thereof changed to the Ca form. The betaine fraction may be concentrated and subjected to crystallization, whereby high-purity betaine can be obtained.
    • PCT No.PCT / JP98 / 05843 Sec。 371日期1999年8月19日 102(e)1999年8月19日PCT 1998年12月24日PCT PCT。 出版物WO99 /​​ 33784 日期1999年7月8日在使用2-组分分离模拟移动床色谱分离器(使用强酸性阳离子交换器)从甜菜提取物或甜菜糖蜜分离和回收蔗糖过程中产生的废物形式的起始溶液材料 树脂为盐形式作为色谱填充)或其浓缩物用于将粗制甜菜碱部分与2-组分分离模拟移动床层析分离器分离,使用与酸性阳离子交换树脂平衡的离子形式的强酸性阳离子交换树脂 起始溶液材料。 使用粗制甜菜碱级分或其浓缩物将其与2-组分分离模拟移动床层析分离器的甜菜碱级分分离,使用色谱填料将具有至少10%(基于离子交换容量)的强酸性阳离子交换树脂 其离子形式变为Ca形式。 可以将甜菜碱级分浓缩并进行结晶,由此可以获得高纯度的甜菜碱。
    • 109. 发明授权
    • Ion chromatographic method and apparatus using ion reflux
    • 离子色谱法和离子回流装置
    • US5914025A
    • 1999-06-22
    • US781537
    • 1997-01-09
    • Hamish Small
    • Hamish Small
    • G01N30/02B01J39/26B01J41/20G01N30/34G01N30/46G01N30/60G01N30/96B01D61/48
    • G01N30/96B01J39/26B01J41/20G01N30/34G01N2030/965G01N30/461
    • A method and apparatus for generating an acid or base eluent in an aqueous stream solely from an ion exchange bed for liquid chromatography of anions or cations and for simultaneously suppressing conductivity of the eluent in the ion exchange bed after chromatographic separation. For a system in which a base is generated for the analysis of anions by ion chromatography, the method uses a bed of cation exchange material with first and second bed sections arranged in series. For anion analysis, the method includes:(a) flowing an aqueous feed stream through the first bed section while applying an electrical potential to form an aqueous eluent stream comprising a cation hydroxide base,(b) flowing a liquid sample stream containing anions to be detected and the eluent through a chromatographic separator portion of said first bed section, to separate said anions to be detected,(c) flowing said aqueous separated anion stream through said second bed section substantially free of anion exchange material and including exchangeable hydronium ions, while applying an electrical potential to convert said base to weakly ionized form, and displacing some of said exchangeable hydronium ions with cations from said base, cations electromigrating from said second bed section to said first bed section in the opposite direction to said aqueous feed stream to replenish exchangeable cations displaced from said first bed in step (a), and(d) flowing said suppressor effluent stream past a detector in which the separated anions in said suppressor effluent are detected.
    • 一种仅在离子交换床中进行阴离子或阳离子液相色谱的含水流中产生酸或碱洗脱液的方法和装置,并同时抑制色谱分离后离子交换床中的洗脱液的电导率。 对于通过离子色谱分析阴离子产生碱的系统,该方法使用具有串联排列的第一和第二床部分的阳离子交换材料床。 对于阴离子分析,所述方法包括:(a)在施加电势的同时使含水进料流流过第一床部分以形成包含阳离子氢氧化物碱的含水洗脱液流,(b)使含有阴离子的液体样品流流动为 检测和洗脱液通过所述第一床部分的色谱分离部分分离,以分离待检测的阴离子,(c)使所述含水分离的阴离子物流通过所述第二床部分基本上不含阴离子交换材料并且包括可交换的水合氢离子,同时 施加电位以将所述碱转化为弱电离形式,以及使来自所述碱的阳离子将一些所述可交换的水合氢离子置换,所述阳离子以与所述含水进料流相反的方向从所述第二床部分电解至所述第一床部分,以补充 在步骤(a)中从所述第一床排出的可交换阳离子,和(d)使所述抑制剂流出物st 通过其中检测到所述抑制流出物中分离的阴离子的检测器。